Solid electrolyte, composite integrated positive electrode, integrated battery and preparation method thereof
A technology of solid electrolyte and electrolyte membrane, which is applied in the field of integrated battery and its preparation, composite integrated positive electrode, and solid electrolyte, which can solve the problems of unstable CNT attachment and easy drop, achieve excellent stability, improve conductivity, and purity high effect
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[0039]The present invention provides a method for preparing a solid electrolyte, which adopts a two-step method of high-temperature solid-phase pre-firing-firing, and includes the following steps:
[0040]S1: Disperse powdered lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide in isopropanol according to a predetermined ratio, and ball mill for 8-12h at 300-400rpm to obtain slurry ; Then, the ground slurry is vacuum dried at 70-90° C. for 10-15h to obtain a mixed powder;
[0041]S2, pre-fired the mixed powder prepared in step S1 at 940-960°C for 4-8 hours to obtain a pre-fired powder, and then subject the pre-fired powder to grinding treatment;
[0042]S3, the pre-fired powder after the grinding treatment in step S2 is fired at 1050 to 1150°C for 12 to 16 hours to obtain the solid electrolyte.
[0043]As a further improvement of the present invention, the mass ratio of lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide is (0.36 to 0.43):...
Embodiment 1
[0053]1. Solid electrolyte Li6.7La3Zr1.7Ta0.3O12(LLZTO) Synthesis:
[0054]It is prepared by a two-step method of high-temperature solid phase pre-firing-firing, including the following steps:
[0055]S1, according to the mass ratio of 0.36:1:0.43:0.14, put powdered lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide into the agate ball mill tank, and use isopropanol as the dispersion liquid. Ball milling at a speed of 350 rpm for 10 hours to obtain a slurry; then, putting the milled slurry in a vacuum oven at 80° C. for vacuum drying for 12 hours to obtain a mixed powder;
[0056]S2, placing the mixed powder prepared in step S1 in a corundum crucible, pre-fired at 950°C for 6 hours (air atmosphere) to obtain a pre-fired powder, and then subject the pre-fired powder to grinding treatment;
[0057]S3, the pre-fired powder after the grinding treatment in step S2 is fired at 1100° C. for 14 hours to obtain LLZTO powder, which is the solid electrolyte.
[0058]2. Preparatio...
Embodiment 2-3
[0091]The difference from embodiment 1 is that in the LLZTO / PVDF composite polymer electrolyte membrane, the mass ratio of LLZTO and PVDF is different, and the other steps are the same as those in uniform embodiment 1, and will not be repeated here.
[0092]Table 2 shows the process parameter settings and performance parameters in Examples 1-3
[0093] Example Mass ratio of LLZTO and PVDF Conductivity Example 1 12:5.146.4×10 -4 S·cm -1
[0094]It can be seen from Table 2 that the influence of the mass ratio of LLZTO and PVDF on the conductivity of the composite polymer electrolyte membrane is: the higher the relative content of LLZTO, the higher the conductivity, but when it increases to a certain value (the mass ratio of LLZTO and PVDF is about 12: 5.14), the conductivity increase is not obvious.
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